Quantification of Representative Ciguatoxins in the Pacific Using Quantitative Nuclear Magnetic Resonance Spectroscopy.
Quantification of Representative Ciguatoxins in the Pacific Using Quantitative Nuclear Magnetic Resonance Spectroscopy.
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DOI：
10.3390/md15100309
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发表时间：
2017-10-12
期刊：
影响因子：
5.4
通讯作者：
Yasumoto T
中科院分区：
文献类型：
--
作者：
Kato T;Yasumoto T
通过定量 1H-NMR 对太平洋雪卡鱼中毒 (CFP) 中涉及的五种毒素进行了绝对定量。目标毒素是雪卡毒素-1B (CTX1B)、52-epi-54-脱氧雪卡毒素-1B (epideoxyCTX1B)、雪卡毒素-3C (CTX3C)、51-羟基雪卡毒素-3C (51OHCTX3C) 和雪卡毒素-4A (CTX4A)。我们首先使用经过认证的标准物质 1,4-BTMSB-d4 校准吡啶-d5 的残留质子，用校准后的吡啶-d5 制备毒素溶液，测量 1H-NMR 谱，并使用校准的残留质子作为内标对毒素进行定量。通过比较目标毒素的选定质子与校准的吡啶-d5 的残留质子之间的信号强度来进行绝对定量。用于定量的雪卡毒素 (CTX) 上的质子信号是经过精心挑选的，这些信号与包括杂质在内的相邻信号完全分离，并且表现出有效强度。为了量化 CTX1B 及其同系物，判断侧链中的烯烃质子是否适合使用。使用纳摩尔溶液可以实现定量。根据各自的毒素计算，不确定性的可能误差在 3% 到 16% 之间。从而避免了珍贵毒素被非挥发性内标污染。吡啶-d5 蒸发后，校准后的 CTX 即可用作 LC/MS 定量分析雪卡毒素的参考标准。
The absolute quantification of five toxins involved in ciguatera fish poisoning (CFP) in the Pacific was carried out by quantitative 1H-NMR. The targeted toxins were ciguatoxin-1B (CTX1B), 52-epi-54-deoxyciguatoxin-1B (epideoxyCTX1B), ciguatoxin-3C (CTX3C), 51-hydroxyciguatoxin-3C (51OHCTX3C), and ciguatoxin-4A (CTX4A). We first calibrated the residual protons of pyridine-d5 using certified reference material, 1,4-BTMSB-d4, prepared the toxin solutions with the calibrated pyridin-d5, measured the 1H-NMR spectra, and quantified the toxin using the calibrated residual protons as the internal standard. The absolute quantification was carried out by comparing the signal intensities between the selected protons of the target toxin and the residual protons of the calibrated pyridine-d5. The proton signals residing on the ciguatoxins (CTXs) to be used for quantification were carefully selected for those that were well separated from adjacent signals including impurities and that exhibited an effective intensity. To quantify CTX1B and its congeners, the olefin protons in the side chain were judged appropriate for use. The quantification was achievable with nano-molar solutions. The probable errors for uncertainty, calculated on respective toxins, ranged between 3% and 16%. The contamination of the precious toxins with nonvolatile internal standards was thus avoided. After the evaporation of pyridine-d5, the calibrated CTXs were ready for use as the reference standard in the quantitative analysis of ciguatoxins by LC/MS.
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影响因子：
4.2
作者：
Ikehara T;Kuniyoshi K;Oshiro N;Yasumoto T
通讯作者：
Yasumoto T
影响因子：
1.8
作者：
SATAKE, M;MURATA, M;YASUMOTO, T
通讯作者：
YASUMOTO, T
影响因子：
2.4
作者：
Saito, T;Nakaie, S;Maeda, T
通讯作者：
Maeda, T
影响因子：
15
作者：
MURATA, M;LEGRAND, AM;YASUMOTO, T
通讯作者：
YASUMOTO, T
影响因子：
0.9
作者：
Saito, Takeshi;Ihara, Toshihide;Hirai, Tetsuya
通讯作者：
Hirai, Tetsuya